Sulfuric Acid → HCID 54535266, compound

HRID 268326Notes

Reaction equation

HRID 268326 reaction equation
[C:1]1([CH:7]([CH3:11])[C:8](O)=[S:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.OS(O)(=O)=O.S(Cl)([Cl:19])=O>C1C=CC=CC=1>[C:1]1([CH:7]([CH3:11])[C:8]([Cl:19])=[S:9])[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1

Participants

5

Reactant 3

HCID 1118Sulfuric AcidHCID 24386Thionyl ChlorideHCID 178460590HCID 178460590, compound

Product 1

HCID 54535266HCID 54535266, compound

Reagents, catalysts & solvents 1

HCID 241BenzeneSolvent

Procedure

In a 500 ml. three-necked reaction flask containing 45 g (247 mmol) of 2-phenylthiopropionic acid (as prepared in example 21) in 280 ml. of anhydrous benzene equipped with a magnetic stirrer, a reflux condenser connected with a wash-bottle containing H2SO4 there are added carefully by a cock-funnel with pressure compensation, 32 g (270 mmol) of thionyl chloride. The mixture is gradually heated until reflux with vigorous stirring. When gas evolution is completed, the solvent is evaporated and the residue is purified by distillation under reduced pressure (106° C/4 mm) to yield 2-phenylthiopropionic acid chloride.

Workup

  1. temperatureThe mixture is gradually heated
  2. temperatureuntil reflux with vigorous stirring
  3. customthe solvent is evaporated
  4. distillationthe residue is purified by distillation under reduced pressure (106° C/4 mm)

Sources & evidence

ORD record
ord-1a29fa5f1a3740a9b14993bc0b44c14c
Source dataset
uspto-grants-1976_03
Patent number
US03947469

Reaction notes

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